Sintering of HAp precipitated from solutions containing ammonium nitrate and PVA
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Sintering of HAp precipitated from solutions containing ammonium nitrate and PVA Tatiana V. Safronova1, Valery I.Putlayev1, Alexey V.Belyakov2, Mikhail A. Shekhirev3 Chemical Department and 3Department of Materials Science of Moscow State University, Leninskie Gory, 1, Moscow 119992, Russia 2 Department of Chemical Thecnology of Silicates of Mendeleev Chemical Technological University of Russia, Miusskaya pl., 9, Moscow 125047, Russia 1
ABSTRACT Bioceramics based on hydroxyapatite (HAp) is known to be a prospective material for biomedical applications. However, sintering of HAp is still understudied in sense of reasonable selection of controlling parameters. In particular, the role of impurities and co-products of powder fabrication is still questionable. The data concerning the role of ammonium nitrate coming to precipitated HAp from the mother liquor, its effect on powder compaction and subsequent sintering, are not available. Nanosized powders of HAp were fabricated via conventional wet-precipitation technique by dropwise adding of Ca(NO3)2 solution (0.25 -1.67 M) to the stock solution of (NH4)2HPO4 (0.15-1.00 M) with pre-adjusted pH at 60 C in presence of polyvinyl alcohol (PVA). PVA was added to the stock solution in order (i) to block crystal growth during synthesis , (ii) to improve stability of Hap suspension to sedimentation, (iii) to regulate an aggregation of HA nanoparticles during synthesis and in the stage of drying. NH4NO3 – a by-product of the precipitation reaction, presented in as-precipitated powder in amount of 30%, was evaluated as an additive affecting a compaction of the powder and the initial stage of a sintering. The powder samples were tested by XRD, FTIR, light-scattering , TEM and SEM/EDX to get particle sizes, morphology and chemical composition, dilatometry. Ceramics were sintered at 700-1250 C and evaluated with SEM/EDX and density measurements. Addition of PVA to the stock solution in the course of HAp precipitation is a promising technique to control an aggregation of HAp nanoparticles in the stages of drying and sintering. PVA acting as a surfactant in the solution and as a binder in dry powder can keep highly reactive small HAp particles within large agglomerates providing better molding of the powder and controllable densification of ceramics. The effect of PVA on microstructure of the HAp powder and their sintering behaviour is discussed in terms of self-organisation concept and synergetics. INTRODUCTION Ceramics based on calcium phosphates is known to be a prospective material for biomedical applications [1]. Much attention is paid to hydroxyapatite Ca10(PO4)6(OH)2 (HAp) due to its affinity to a bone mineral. Different precursors have been used to synthesize HAp powders. The most popular reaction consists in precipitation from (NH4)2HPO4 and Ca(NO3)2 solutions. Effect of the principal parameters of the powder fabrication on sintering was extensively discussed (see, e.g., [2]). However, the role of impurities and co-products of powder fabrication is still question
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